CN105403523A - Method for determining chlorine in titanium sponge, titanium and titanium alloy - Google Patents
Method for determining chlorine in titanium sponge, titanium and titanium alloy Download PDFInfo
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- CN105403523A CN105403523A CN201510706742.0A CN201510706742A CN105403523A CN 105403523 A CN105403523 A CN 105403523A CN 201510706742 A CN201510706742 A CN 201510706742A CN 105403523 A CN105403523 A CN 105403523A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
Abstract
The invention belongs to the technical field of analytical chemistry, and relates to a method for determining chlorine in titanium sponge, titanium and titanium alloy. The method comprises the following steps: weighing a sample material, adding hydrofluoric acid to dissolve the sample material, adding nitric acid, stirring until the obtained solution is colorless, adding boric acid, fully stirring, adding a solvent to a constant volume, and shaking up to obtain a sample material solution; and taking the sample material solution, sequentially adding nitric acid and water, uniformly mixing, adding 0.50-3.00mL of acetone, mixing for 10-60min, adding 0.50-3.00mL of silver nitrate, uniformly mixing, diluting, carrying out constant temperature heating, cooling to room temperature, measuring the turbidity value of the obtained sample solution in a 3cm colorimetric ware at 420nm, and solving the content of chloride ions from a working curve. The method has the advantages of high accuracy and precision of a measured value, large detection range and high feasibility.
Description
Technical field
The invention belongs to technical field of analytical chemistry, relate to the assay method of chlorine in a kind of titanium sponge, titanium or titanium alloy.
Background technology
Titanium sponge, titanium or titanium alloy have the features such as density is little, physical strength is large, rotproofness is good, non magnetic, linear expansion coefficient is little, are widely used in the fields such as aviation, navigation, chemical industry, oil, weaving, medicine equipment.
Find according to the study, when in titanium material, chlorinity is higher, titanium material there will be " blackspot " phenomenon, time serious, surface can produce the globule or be corroded, so, reduce chlorinity in titanium material, to titanium material, there is important practice significance, thus, chlorinity in Accurate Determining titanium sponge, titanium or titanium alloy, has extremely important effect to titanium or titanium alloy production, the development of titanium material etc.
At present, in titanium sponge, titanium or titanium alloy, the assay method of chlorine is mainly silver sulfide spectrophotometric method and ion selective electrode method, but these two kinds of methods analyst long flow paths, analysis speed are slow, be unfavorable for that titanium sponge, titanium or titanium alloy are produced in batches, for this reason, the present invention adopts silver chloride nephelometry to provide a kind of new approaches for measuring chlorinity in titanium sponge, titanium or titanium alloy.
Summary of the invention
The object of the present invention is to provide a kind of simple to operation, analysis result assay method of chlorine in titanium sponge, titanium or titanium alloy accurately.
Be achieved especially by following scheme:
First, the span of correlation parameter and the influence factor to assay method is determined by experiment.
Step 1: analytical wavelengths is determined
Get 10.00mL chlorine standard solution and be placed in the brown volumetric flask of 50mL, add 4.00mL nitric acid, after 25.00mL water stirs, after adding 1.00mL acetone mix and blend 20min, add 1.00mL silver nitrate and stir, be diluted with water to 50.00mL, at temperature is 70 DEG C, after heated at constant temperature 10min, put into cold water and be cooled to room temperature, use 3cm cuvette, measure by the spectrophotometric using method of tradition, the results are shown in Figure 1, the maximum absorption band of silver chloride is positioned at 420nm place as seen from Figure 1.
Step 2: the selection of response parameter and the analysis of disturbing factor
Step 2.1: the selection of acetone consumption
Adopt 10mL transfer pipet to pipette 6 parts of chlorine standard solution and be placed in the brown volumetric flask of 50mL, after every part all adds 4.00mL nitric acid, 25.00mL water stirs, add 0.50 respectively, 1.00,1.50,2.00,2.50,3.00mL acetone, and after mix and blend 20min, add 1.00mL silver nitrate to stir, be diluted with water to
50.00mL, at temperature is 70 DEG C after heated at constant temperature 10min, put into cold water and be cooled to room temperature, use 3cm cuvette, measure by the spectrophotometric using method of tradition, the results are shown in Figure 2, acetone consumption is in 0.50-3.00mL as seen from Figure 2, little to absorbance change, the most stable when consumption is 1.00mL.
Step 2.2: the determination adding incorporation time after acetone
Adopt 10mL transfer pipet to pipette 6 parts of chlorine standard solution and be placed in the brown volumetric flask of 50mL, every part all adds 4.00mL nitric acid, after 25.00mL water stirs, add 1.00mL acetone, mix and blend 10 respectively, 20, 30, 40, 50, after 60min, add after 1.00mL silver nitrate stirs, be diluted with water to 50.00mL, at temperature is 80 DEG C after heated at constant temperature 10min, put into cold water and be cooled to room temperature, use 3cm cuvette, measure by the spectrophotometric using method of tradition, the results are shown in Figure 3, after adding acetone mix and blend 20min as seen from Figure 3, material system starts to stablize, illustrate: 20min afterchlorinate silver colloidal suspensions and acetone form uniform mix.
Step 2.3: the selection of silver nitrate consumption
Adopt 10mL transfer pipet to pipette 6 parts of chlorine standard solution and be placed in the brown volumetric flask of 50mL, every part all adds 4.00mL nitric acid, after 25.00mL water stirs, after adding 1.00mL acetone mix and blend 20min, add 0.50 respectively, 1.00, 1.50, 2.00, 2.50, after 3.00mL silver nitrate stirs, be diluted with water to 50.00mL, at temperature is 60 DEG C after heated at constant temperature 15min, put into cold water and be cooled to room temperature, use 3cm cuvette, measure by the spectrophotometric using method of tradition, the results are shown in Figure 4, silver nitrate consumption is less to silver chloride turbidity value determination influences within the scope of 0.50-3.00mL as seen from Figure 4, wherein, when acetone consumption is 1.00mL, turbidity value is the most stable.
Step 2.4: the impact of coexistence elements
Pipette 2 parts of 10.00mL chlorine standard solution and be placed in the brown volumetric flask of 50mL, portion adds pure titanium 10.00mg, another part adds titanium tetrachloride 10.00mg, obtain analog sample, then, add 4.00mL nitric acid, after 25.00mL water stirs, add 1.00mL acetone mix and blend 20min, add 1.00mL silver nitrate to stir, be diluted with water to 50.00mL, at temperature is 70 DEG C after heated at constant temperature 10min, put into cold water and be cooled to room temperature, use 3cm cuvette, measure by the spectrophotometric using method of tradition, result is as Fig. 5, shown in Fig. 6, by Fig. 5, the visible titanium of Fig. 6, molybdenum, vanadium, zirconium, aluminium, tin, nickel, manganese, copper, neodymium, tungsten, palladium, ruthenium, silicon equal size does not all disturb silver chloride turbidity value to measure.
Step 3: the drafting of working curve
Pipette chlorine standard solution 0 respectively, 1.00, 2.00, 3.00, 4.00, 5.00mL is in 6 brown volumetric flasks of 50mL, every part all adds 4.00mL nitric acid, after 25.00mL water stirs, add 0.50-3.00mL acetone mix and blend 10-60min, add 0.50-3.00mL silver nitrate to stir, be diluted with water to 50.00mL, after heated at constant temperature 8-15min, put into cold water and be cooled to room temperature, with not chloride standard solution for reference liquid, the turbidity value recorded with 3cm cuvette is to chlorinity drawing curve corresponding in solution, wherein, response parameter and consumption as shown in table 1, result as shown in Figure 7, as seen from Figure 7, cl concn is in 0-180 μ g/50mL, this result meets Beer law, can obtain thus, x=0.002448y-0.00116 ((as x < 0.2) or y=400x+4 (when >=0.2), wherein, x represents turbidity value, y represents 50mL turbidimetric analysis turbidimetry Chlorine in Solution content, coefficient R is 0.9997.
Table 1
Step 4: the mensuration of the recovery
(1) 1.00-2.00g test portion is taken in 250mL tygon beaker, add water, each 5.00mL of hydrofluorite, and be stirred to sample and dissolve completely, add 10.00mL nitric acid, and be stirred to solution without any colour generation, add 2g boric acid and stir fully, move in 100mL volumetric flask, constant volume, shakes up, and obtains sample solution; Blank test is done in company with test portion;
Get 5.00-20.00mL sample solution and be placed in the brown volumetric flask of 50mL, get 7 parts altogether, add the pure silicon of 2.00,4.00,6.00,8.00,10.00,14.00,16.00 μ g respectively, then 4.00mL nitric acid is added, after 25.00mL water stirs, add 0.50-3.00mL acetone mix and blend 10-60min, add 0.50-3.00mL silver nitrate to stir, be diluted with water to 50.00mL, after heated at constant temperature 8-15min, put into cold water and be cooled to room temperature, use 3cm cuvette, with blank for reference liquid in company with test portion
,turbidity value is measured in 420nm place.
Step 5: the mensuration of accuracy
(2) 1.00-2.00g test portion is taken in 250mL tygon beaker, add water, each 5.00mL of hydrofluorite carries out being stirred to sample and dissolve completely, add 10.00mL nitric acid, and it is colourless to be stirred to solution, add 2g boric acid to stir fully, move in 100mL volumetric flask, constant volume, shake up, obtain sample solution; Blank test is done in company with test portion;
(3) get 5.00-20.00mL sample solution and be placed in the brown volumetric flask of 50mL, add 4.00mL nitric acid successively, after 25.00mL water stirs, add 0.50-3.00mL acetone mix and blend 10-60min, add 0.50-3.00mL silver nitrate to stir, be diluted with water to 50.00mL, after heated at constant temperature 8-15min, put into cold water and be cooled to room temperature, use 3cm cuvette, with blank for reference liquid in company with test portion
,turbidity value is measured in 420nm place, according to x=0.002448y-0.00116 (as x < 0.2) or y=400x+4 (when>=0.2), wherein, x represents turbidity value, y represents 50mL turbidimetric analysis turbidimetry Chlorine in Solution content, tries to achieve chlorinity in sample.
Described water is secondary or the above water of secondary, and hydrofluorite, that boric acid is top grade is pure, and acetone is pure for analyzing.
Described chlorine concentration of standard solution is 10 μ g/mL.
Described nitric acid, its pH is 0.046-0.52, and its concentration of volume percent is 50%.
Described silver nitrate concentration is 10
4μ g/mL.
Described heated at constant temperature temperature is 60-80 DEG C, and preferred heated at constant temperature temperature is 70 DEG C.
Beneficial effect of the present invention
Adopt silver chloride nephelometry, its method is simple, analysis speed is fast, not by the interference of the elements such as titanium, molybdenum, vanadium, aluminium, tin, nickel, manganese, copper, silicon, especially titanium on the mensuration of chlorine almost without impact, the lower limit that detects of the inventive method is 0.01%, the recovery is about 98.0-100.5%, coefficient R is 0.9997, according to the testing result of embodiment 1-7, calculating its standard deviation is 0.014, its relative standard deviation is less than 7%, illustrate the inventive method accuracy and precision high, sensing range is larger.
Accompanying drawing explanation
Fig. 1: silver chloride absorption curve
Fig. 2: the graph of a relation of acetone consumption gradient and absorbance
Fig. 3: acetone adds the graph of a relation of rear incorporation time and absorbance
Fig. 4: the graph of a relation of silver nitrate consumption gradient and absorbance
Fig. 5: containing the silver chloride absorption curve of pure titanium
Fig. 6: containing the silver chloride absorption curve of titanium tetrachloride
Fig. 7: working curve
Embodiment
Below in conjunction with concrete embodiment, further restriction is done to technical scheme of the present invention, but claimed scope is not only confined to done description.
Embodiment 1
An assay method for chlorine in titanium sponge, titanium or titanium alloy, comprises the following steps:
(1) title 1.85g titanium sponge is got in 250mL tygon beaker, add water, each 5.00mL of hydrofluorite, and be stirred to sample and dissolve completely, add 10.00mL nitric acid, and be stirred to solution without any colour generation, add 2g boric acid and stir fully, move in 100mL volumetric flask, constant volume, shakes up, and obtains sample solution; Blank test is done in company with test portion;
(2) get 20.00mL sample solution and be placed in the brown volumetric flask of 50mL, add 4.00mL nitric acid successively, after 25.00mL water mixes, add 0.50mL acetone mix and blend 60min, add 0.50mL silver nitrate to stir, be diluted with water to 50.00mL, at constant temperature is 78 DEG C after heating water bath 10min, puts into cold water and be cooled to room temperature, use 3cm cuvette, with blank for reference liquid in company with test portion
,measure turbidity value in 420nm place, its turbidity value is 0.21, calculates in 50mL turbidimetric analysis turbidimetry solution containing 86 μ g chlorine.
Described water is secondary or the above water of secondary, and hydrofluorite, that boric acid is top grade is pure, and acetone is pure for analyzing.
Described nitric acid, its pH is 0.50, and its concentration of volume percent is 50%.
Described silver nitrate concentration is 10
4μ g/mL.
Embodiment 2
An assay method for chlorine in titanium sponge, titanium or titanium alloy, comprises the following steps:
(1) title 1.50g titanium alloy is got in 250mL tygon beaker, add water, each 5.00mL of hydrofluorite, and be stirred to sample and dissolve completely, add 10.00mL nitric acid, and be stirred to solution without any colour generation, add 2g boric acid and stir fully, move in 100mL volumetric flask, constant volume, shakes up, and obtains sample solution; Blank test is done in company with test portion;
(2) get 5.00mL sample solution and be placed in the brown volumetric flask of 50mL, add 4.00mL nitric acid successively, after 25.00mL water stirs, add 2.00mL acetone mix and blend 25min, add 1.50mL silver nitrate to stir, be diluted with water to 50.00mL, at constant temperature is 65 DEG C after microwave heating 8min, puts into cold water and be cooled to room temperature, use 3cm cuvette, with blank for reference liquid in company with test portion
,measure turbidity value in 420nm place, its turbidity value is 0.23, calculates in 50mL turbidimetric analysis turbidimetry solution containing 94 μ g chlorine.
Described water is secondary or the above water of secondary, and hydrofluorite, that boric acid is top grade is pure, and acetone is pure for analyzing.
Described nitric acid, its pH is 0.048, and its concentration of volume percent is 50%.
Described silver nitrate concentration is 10
4μ g/mL.
Embodiment 3
An assay method for chlorine in titanium sponge, titanium or titanium alloy, comprises the following steps:
(1) title 1.00g titanium material is got in 250mL tygon beaker, add water, each 5.00mL of hydrofluorite, and be stirred to sample and dissolve completely, add 10.00mL nitric acid, and be stirred to solution without any colour generation, add 2g boric acid and stir fully, move in 100mL volumetric flask, constant volume, shakes up, and obtains sample solution; Blank test is done in company with test portion;
(2) get 15.00mL sample solution and be placed in the brown volumetric flask of 50mL, add 4.00mL nitric acid successively, after 25.00mL water stirs, add 1.50mL acetone mix and blend 30min, add 1.00mL silver nitrate to stir, be diluted with water to 50.00mL, at constant temperature is 80 DEG C after heating water bath 15min, put into cold water and be cooled to room temperature, use 3cm cuvette, with blank for reference liquid in company with test portion, measure turbidity value in 420nm place, its turbidity value, for being 0.19, calculates in 50mL turbidimetric analysis turbidimetry solution containing 78 μ g chlorine.
Described water is secondary or the above water of secondary, and hydrofluorite, that boric acid is top grade is pure, and acetone is pure for analyzing.
Described nitric acid, its pH is 0.22, and its concentration of volume percent is 50%.
Described silver nitrate concentration is 10
4μ g/mL.
Embodiment 4
On the basis of embodiment 1, get 10.00mL sample solution and measure, its turbidity value is 0.22, calculates in 50mL turbidimetric analysis turbidimetry solution containing 90 μ g chlorine.
Embodiment 5
On the basis of embodiment 2, get 15.00mL sample solution and measure, its turbidity value is 0.23, calculates in 50mL turbidimetric analysis turbidimetry solution containing 94 μ g chlorine.
Embodiment 6
On the basis of embodiment 3, get 20.00mL sample solution and measure, its turbidity value is 0.20, calculates in 50mL turbidimetric analysis turbidimetry solution containing 82 μ g chlorine.
Embodiment 7
On the basis of embodiment 1, get 8.00mL sample solution and measure, its turbidity value is 0.21, calculates in 50mL turbidimetric analysis turbidimetry solution containing 86 μ g chlorine.
Test example 1
The method utilizing mark-on to reclaim carries out the calculating of the test portion recovery, according to above-mentioned determination of recovery rates method, on embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6, embodiment 7 basis, add the chlorine of 2.00 μ g, 4.00 μ g, 6.00 μ g, 8.00 μ g, 10.00 μ g, 14.00 μ g, 16.00 μ g respectively, its result is as shown in table 2:
Table 2
| Add Cl (μ g) | 2.00 | 4.00 | 6.00 | 8.00 | 10.00 | 14.00 | 16.00 |
| Record Cl (μ g) | 2.01 | 3.97 | 5.9 | 8.03 | 9.8 | 13.88 | 15.69 |
| The recovery (%) | 100.5 | 99.5 | 98.3 | 100.4 | 98.0 | 99.14 | 98.1 |
2, as shown in Table 2, the recovery, between 98.0-100.5%, illustrates, this method recovery is higher.
Claims (7)
1. the assay method of chlorine in titanium sponge, titanium or titanium alloy, is characterized in that, comprise the following steps:
(1) 1.00-2.00g test portion is taken in 250mL tygon beaker, add water, each 5mL of hydrofluorite, and be stirred to after sample dissolves completely, add 10.00mL nitric acid, and be stirred to solution without any colour generation, add 2g boric acid and stir fully, move in 100mL volumetric flask, constant volume, shakes up, and obtains sample solution; Blank test is done in company with test portion;
(2) get 5.00-20.00mL sample solution and be placed in the brown volumetric flask of 50mL, add 4.00mL nitric acid successively, after 25.00mL water stirs, add 0.50-3.00mL acetone mix and blend 10-60min, add 0.50-3.00mL silver nitrate to stir, be diluted with water to 50.00mL, after heated at constant temperature 8-15min, be cooled to room temperature, use 3cm cuvette, with blank for reference liquid in company with test portion
,turbidity value is measured in 420nm place, according to x=0.002448y-0.00116 (as x < 0.2) or y=400x+4 (when>=0.2), wherein, x represents turbidity value, y represents 50mL turbidimetric analysis turbidimetry Chlorine in Solution content, tries to achieve chlorinity in sample.
2. titanium sponge as claimed in claim 1, the assay method of chlorine in titanium or titanium alloy, it is characterized in that, described working curve plot step is: get chlorine standard solution 0 respectively, 1.00, 2.00, 3.00, 4.00, 5.00mL is in 6 brown volumetric flasks of 50mL, 4.00mL nitric acid is added successively in each volumetric flask, after 25.00mL water mixes, add 0.50-3.00mL acetone mixing 10-60min, add 0.50-3.00mL silver nitrate to mix, be diluted with water to 50.00mL, after heated at constant temperature 8-15min, be cooled to room temperature, with not chloride standard solution for reference liquid, the turbidity value recorded with 3cm cuvette is to chlorinity drawing curve corresponding in solution, coefficient R is 0.9997.
3. the assay method of chlorine in titanium sponge as claimed in claim 1, titanium or titanium alloy, it is characterized in that, described heated at constant temperature temperature is 60-80 DEG C.
4. in the titanium sponge as described in claim 1 or 3, titanium or titanium alloy, the assay method of chlorine, is characterized in that, described heated at constant temperature temperature is 70 DEG C.
5. the assay method of chlorine in titanium sponge as claimed in claim 1, titanium or titanium alloy, it is characterized in that, described nitric acid, its pH is 0.046-0.52, and its concentration of volume percent is 50%.
6. the assay method of chlorine in titanium sponge as claimed in claim 1, titanium or titanium alloy, it is characterized in that, the concentration of described silver nitrate is 10
4μ g/mL.
7. the assay method of chlorine in titanium sponge as claimed in claim 1, titanium or titanium alloy, it is characterized in that, the concentration of described chlorine standard solution is 10 μ g/mL.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106018401A (en) * | 2016-06-29 | 2016-10-12 | 湖南省湘维有限公司 | Method for determining content of chlorine ions in water |
| CN106770408A (en) * | 2017-01-05 | 2017-05-31 | 国家电网公司 | The detection method of corrosivity chlorinity in a kind of fire-resistance oil |
| CN108593574A (en) * | 2018-04-09 | 2018-09-28 | 西部矿业股份有限公司 | A kind of method of chlorinity in measurement zinc concentrate |
| CN109444063A (en) * | 2018-12-21 | 2019-03-08 | 广西川金诺化工有限公司 | A method of trace chlorine content in measurement commercial wet process purifying phosphoric acid |
| CN110361339A (en) * | 2019-05-31 | 2019-10-22 | 衢州康鹏化学有限公司 | The detection method of chloride in imidodisulfuryl fluoride lithium salt |
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2015
- 2015-10-27 CN CN201510706742.0A patent/CN105403523A/en active Pending
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106018401A (en) * | 2016-06-29 | 2016-10-12 | 湖南省湘维有限公司 | Method for determining content of chlorine ions in water |
| CN106770408A (en) * | 2017-01-05 | 2017-05-31 | 国家电网公司 | The detection method of corrosivity chlorinity in a kind of fire-resistance oil |
| CN106770408B (en) * | 2017-01-05 | 2019-09-27 | 国家电网公司 | The detection method of corrosivity chlorinity in a kind of fire-resistance oil |
| CN108593574A (en) * | 2018-04-09 | 2018-09-28 | 西部矿业股份有限公司 | A kind of method of chlorinity in measurement zinc concentrate |
| CN109444063A (en) * | 2018-12-21 | 2019-03-08 | 广西川金诺化工有限公司 | A method of trace chlorine content in measurement commercial wet process purifying phosphoric acid |
| CN110361339A (en) * | 2019-05-31 | 2019-10-22 | 衢州康鹏化学有限公司 | The detection method of chloride in imidodisulfuryl fluoride lithium salt |
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